Method of producing resin soap



Patented May 20, 1941 mz'rnon or raonvcmo aasm soar Arthur Langmeier, Wilmington. Del., assignor to Hercules Powder Company, Wilmington, Del., a corporation of Delaware No Drawing. Application October 25, 1931;, Serial No. 230,895

6 Claims.

This invention relates to an improved method for the preparation of soap made from the resin obtained as a by-product in the refining of FF wood rosin to a pale grade of wood rosin.

Heretofore, it has been known to produce a soap by saponlfication oi rosin with an alkali in liquid, aqueous medium at temperatures of approximately 100 C. In such a process the viscosity of the soap from the resin obtained as a by-product in the refining of FF wood rosin is quite high due to the high melting point of the resin. The high viscosity renders adequate mixing and control difiicult.

Now, in accordance with this invention, I have found that I may produce substantially neutral soap from the resin obtained as a by-product in the refining of FF wood rosin by a much simpler process than has hitherto been used. According to my process, the soap is produced without the use of heat.

The resin obtained as a by-product in the refining of FF wood rosin which I employ in my improved method of preparation of soap therefrom is hereby defined as the dark-colored, hard resin that is obtained as a by-product when FF wood rosin is dissolved in a suitable solvent, such as a volatile petroleum hydrocarbon, and refined to pale grades oi wood rosin by any of the methods known to the art.

Thus, the resin may be, more specifically, the dark-colored resin obtained as a by-product when FF wood rosin is dissolved in a low boiling petroleum hydrocarbon and refined to pale grades of wood rosin by treatment with furfural. Other refining agents such as, for example, fullers earth, phenol, sulfur dioxide, chlorohydrin, furfuryl alcohol, resorcinol, etc... may be used. The resin may also be obtained as the distillation residue in the distillation of FF wood rosin to produce pale grades of wood rosin. The by-product resin will have the following approximate analysis:

Acid number 105-140 Sapon. number 150-170 M. P. (Hercules drop method) degrees Fahrenheit 175-210 Unsaponifiahle per cent" 10-20 Gasoline insoluble do 30-80 Petroleum ether insoluble -do 30-80 ably finer than 50 mesh. The process is carried out in two stages.

In the first stage the pulverized hy-product resin is dispersed in cold water. Dispersion may be accomplished in any convenient manner, such as by addition of a small amount of alkali to the water, say about 2 to about 10 per cent of the alkali required for saponification of the resin. Likewise, the pulverized resin may be dispersed in the water with any suitable dispersing agent, such as, for example, a solution of casein in sodium hydroxide, sodium oleate, sodium alginate, triethanolamine oleate, sulfated higher alcohols, sulfonated higher alcohols, sulionated naphthalenes, bentonite, pine oil, etc. The pulverized by-product resin may also be dispersed in water mechanically without the use of agents as above. Such mechanical dispersion may be accomplished by making a heavy paste of about or more pulverized by-product resin and water. in a suitable type of mixer, adding water and mixing until a smooth paste results. Dilution of the smooth paste to lower solids content is then preferable for convenience of handling in the subsequent operation.

The above dispersion of the by-product resin in water may be carried out over a wide range of concentration. I have prepared satisfactory dispersions in concentrations of about 10 per cent to about 50 per cent by weight, but prefer to carry out the dispersion with about 20 to about 40 per cent solids.

In the second stage the pulverized by-product resin dispersed in water as described above is saponified with alkali without the use of heat. The saponification is carried out by addition of a concentrated alkali solution, such as a solution of an alkali metal hydroxide, to the dispersion with mechanical agitation.

Although I have described my procedure as involving first the dispersion of the pulverized by-product resin in water, then the saponiflcation of the resin by addition of alkali, I find that other procedures may be used to produce the same result. Thus, I may saponify the resin by adding it in dry, pulverized form to the alkali solution, thereby dispersing and saponifying the resin in one operation.

As specific examples of my improved method of preparation of soap from the resin obtained as a by-product in the refining of FF wood rosin, the following are illustrative:

Example 1 Forty-five parts by weightoi pulverized resin Per cent Free resin 2.7 Free alkali as NaOH 0.05

Total solids 45.6

Example 2 Twenty-five parts by weight of pulverized resin obtained as a by-product in the refining of FF wood resin were added with agitation to a solution of 0.04 part by weight of sodium hydroxide dissolved in 223 parts by weight of water. After agitation had continued for about two minutes, a solution of 2.1 parts by weight of sodium hydroxide dissolved in 7.9 parts by weight of water was added at room temperature with agitation. After agitation had continued for about 30 minutes the soap was ready for use. It showed the following analysis:

Per cent Fre resin 1,1 Free alkali as NaOH 0.04 Total solids 10.1

Example 3 Fifty parts by weight of pulverized resin obtained as a by-product in the refining of FF wood rosin were added with agitation to a solution of 0.25 part by weight of potassium hydroxide dis solved in 100 parts by weight of water. After agitating for about two minutes, a solution of 6 parts by weight of potassium hydroxide dissolved in 12 parts by weight of water was added at room temperature with agitation. After agitation had continued for about 30 minutes, the by-product resin soap was suitable for use, for example, as a sizing agent for paper. It had the following analysis:

. Per cent Free resin 0.0 Free alkali as KOH 0.35 Total solids 32.3

Y Example 4 30 minutes. The by-product resin soap had the following analysis:

. Per cent Free resin 2.1 Free alkali as NaOH 0.05 Total solids 30.9

Example 5' Fifty parts by weight of pulverized resin obtained as a by-product in the refining of FF wood rosin were dispersed in a mixture of 0.5

part by weight of pine oil and parts by weight of water at room temperature with agitation. A solution of 4.5 parts by weight of sodium hydroxide dissolved in 9 parts by weight of water was then added at room temperature with agitation' After agitation had continued for about 30 minutes the soap had the following analysis:

Per cent Free resin 0.0 Free alkali as NaOH 0.37 Total solids 31.8

In the aboveexamples potassium hydroxide and sodium hydroxide are considered as equivalents, substitution of one for the other being on the basis of equivalent amounts.

In practicing my invention, I prefer to use a concentrated solution of alkali to effect the saponification, as the reaction is more rapid when the concentration of alkali is high. My preferred strength of alkali is'about 20 to about 50 per cent. It will be appreciated, however, that the concentration of alkali is not considered critical, the lower limit being determined by the reactivity with the resin and the upper limit eing dependent on the solution strength which can be conveniently prepared and handled.

The soap solution produced from the resin produced as a by-product in the refining of FF wood rosin in accordance with this invention may be used as a sizing material, such as for sizing of paper and board.

It will be appreciated that the details and proportions set forth in the examples herein are 11- lustrative only, and that the invention as broadly described is in no way limited thereby.

What I claim and desire to protect by Letters Patent is:

l. A method of preparing a soap solution which comprises dispersing in water the resin obtained as a by-product in the refining of FF wood rosin to a pale grade of wood rosin and characterized by an acid number from about to about 140, a saponification number from about to 170, an unsaponifiable content from about 10 to about 20 per cent, a drop melting point from about to about 210 F. and a gasoline insoluble content from about 30 to about 80 per cent, carrying out said dispersion with about 10 to about 50 per cent by weight solids concentration, and saponifying the said resin at room temperature with an aqueous alkali metal hydroxide solution of about 20 to about 50 per cent concentration to give a substantially neutral soap.

2. A method of preparing a soap solution which comprises dispersing in water the resin obtained as a by-product in the refining of FF wood rosin to a pale grade of wood rosin and characterized by an acid number from about 105 to about 140, a saponification number from about 150 to about 170, an unsaponifiable content from about 10 to about 20 per cent, a drop melting point from about 175 to about 210 F. and a gasoline insoluble content from about 30 to about 80 per cent, carrying out said dispersion with about 20 to about 40 per cent by weight solids concentration, and saponifying the said resin at room temperature with an aqueous alkali metal hydroxide solution of about 20 to about 50 per cent concentration to give a substantially neutral soap.

3. A method of preparing a soap solution which comprises dispersing in water the resin obtained as a by-product in the refining of FF wood rosin to a pale grade of wood rosin and characterized by an acid number from about 106 to about 140,

a saponiiication number from about 150 to about 1'10, an unsaponiilable oontent irom abuit to about per cent, a drop melting point from about 175 to about 210 1''. and a gasoline insoluble content from about to about 80 per cent, carrying out said lii rsion with about 10 to about per cent by weight solids concentration by addition oi alkali, and saponii'ying the said resin at roomtemperature with an aqueous alkali metal hydroxide solution of about 20 to abut 50 per cent concentration to give a substantially neutral soap.

4. A method oi preparing a soap solution which comprises dispersing in water the resin obtained asaby-productinthe-reflningoil 'l'woodroain to'apalegradeolwoodrosinandcheracterised byan acid number irom about 105 to about 140,

. a saponiiication number from about 150 to about l'lman 1e content from about 10 to about 20 per cent, a drop melting point irom about 175'. to about 210 1''. and a gasoline insoluble content from about 30 to about per cent, carrying out said dispersion with about 10 to about 50 per cent by weight solids concentra as a by-product in the refining oi FF wood to a pale grade of woodrosln and characterized by an acid number from about to about 140, a saponiilcation number from about to about 170, an unsaponiflable content from about 10 to about 20 per cent, a drop melting point from about to about 210 F. and asasoline insoluble content from about 30 to about 80 per cent, carrying out said dispersion with about 10 to about 50 per cent by weight solids concentration, and saponiiying the said resin at room temperature with an aqueous sodium hydroxide solution of about 20 to about 50 per cent concentration to give a substantially neutral soap.

6. A method of preparinga soap solution which comprises dispersing in water the resin obtained as a by-product in the refining of FF wood rosin to a pale grade of wood rosin and characterized by an acid number from about 105 to about-140, a saponiiication number from about 150 to about 170, an unsaponiflable content from about 10 to about 20 per cent, a drop melting point trom about 175 to about 210 F. and a gasoline insoluble content from about 30 to about 80 per cent, carrying out said dispersion with about 10 to about 50 per cent by weight solids concentration, and saponii'ying the said resin at room temperature with an aqueous potassium hydroxide solution of about 20 to about 50 per cent concentration to give a substantially neutral soap.

ARTHUR. LANGMEIER. 

